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NIST Special Publication 1233
NIST Nanotechnology
Environmental, Health, and Safety
Research Program: 2009–2016
Debra L. Kaiser
Vincent A. Hackley
This publication is available free of charge from:
https://doi.org/10.6028/NIST.SP.1233
NIST Special Publication 1233
NIST Nanotechnology
Environmental, Health, and Safety
Research Program: 2009–2016
Debra L. Kaiser
Office of Data and Informatics
Material Measurement Laboratory
Vincent A. Hackley
Materials Measurement Science Division
Material Measurement Laboratory
This publication is available free of charge from:
https://doi.org/10.6028/NIST.SP.1233
November 2018
U.S. Department of Commerce
Wilbur L. Ross, Jr., Secretary
National Institute of Standards and Technology
Walter Copan, NIST Director and Under Secretary of Commerce for Standards and Technology
Certain commercial entities, equipment, or materials may be identified in this
document in order to describe an experimental procedure or concept adequately.
Such identification is not intended to imply recommendation or endorsement by the
National Institute of Standards and Technology, nor is it intended to imply that the
entities, materials, or equipment are necessarily the best available for the purpose.
National Institute of Standards and Technology Special Publication 1233
Natl. Inst. Stand. Technol. Spec. Publ. 1233, 55 pages (November 2018)
CODEN: NSPUE2
This publication is available free of charge from:
https://doi.org/10.6028/NIST.SP.1233
i
Abstract
In response to needs of a government-wide initiative in nanotechnology led by a
subcommittee within the White House’s Office of Science and Technology Policy, NIST
established a nanotechnology environmental, health, and safety (nano-EHS) research
program in 2009 that remained active through 2016. This document summarizes the
NIST Nano-EHS Program goals, projects, outputs, and impacts. The program was
designed to address, in collaboration with other agencies, the research needs for a
comprehensive U.S. measurement infrastructure for nano-EHS as identified by federal
agencies participating in the National Nanotechnology Initiative. Such an infrastructure
included a suite of measurement tools—methods, protocols, standards (reference
materials and documentary), instruments, models, and benchmark (validated) data. The
NIST Nano-EHS Program made substantial progress in developing the required
infrastructure, producing 9 reference materials, 24 web-accessible protocols, and 212
archival journal articles, 59% of which have been published in journals with impact
factors greater than 3. In addition, program team members held leadership positions in
the nanotechnology committees of major standards development organizations and led
and contributed to the development of standards in these committees.
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Table of Contents
1. Introduction ...................................................................................................................1
1.1. What is Nano-EHS? ..............................................................................................1
1.2. The National Nanotechnology Initiative and Nano-EHS .....................................1
1.3. The NIST Role in Federal Nano-EHS Efforts ......................................................2
2. History of the NIST Nano-EHS Program ...................................................................2
2.1. Biomedical Applications ........................................................................................2
2.2. Nano-EHS Funding ................................................................................................3
2.3. Nano-EHS Program Researchers ...........................................................................3
3. NIST Nano-EHS Program Goals and Projects ..........................................................4
3.1. 2009‒2011..............................................................................................................5
3.2. 2012‒2014..............................................................................................................5
3.2.1. Goal 1 ............................................................................................................5
3.2.2. Goal 2 ............................................................................................................6
3.3. 2015‒2016..............................................................................................................6
4. NIST Nano-EHS Program Outputs ............................................................................7
4.1. Publications ...........................................................................................................7
4.2 Protocols and Assays ............................................................................................7
4.3. Reference Materials ...............................................................................................8
4.4. Documentary Standards .........................................................................................8
5. NIST Nano-EHS Program Impacts ..............................................................................9
5.1. Case Study I: Gold Nanoparticle Reference Materials ..........................................9
5.2. Case Study II: Measurement Assurance for a Nanotoxicity Assay .....................10
6. Conclusions ...................................................................................................................12
Acknowledgements ..........................................................................................................13
References .........................................................................................................................13
Appendix A: Nano-EHS Program Researchers ............................................................15
Appendix B: Nano-EHS Initiative Program Plan, FY12-14 ........................................17
Appendix C: Nano-EHS Program Publications ............................................................23
Appendix D: Nano-EHS Program Protocols and Assays .............................................45
Appendix E: Nanoscale Reference Materials ................................................................49
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List of Tables
Table 1. Designated Nano-EHS funds .................................................................................3
Table 2. Nano-EHS investments reported to the NNI .........................................................3
Table 3. Number of publications per JIF range ...................................................................7
Table 4. Purchasers of RM 8012 as of September 5015 ....................................................10
List of Figures
Fig. 1. Interrelationships of the five core research areas .....................................................2
Fig. 2. Units of RMs 8011, 8012, and 8013 .........................................................................9
Fig. 3. Number of publications by year .............................................................................10
Fig. 4. 96-well plate layout for cytotoxicity assays on ENMs ...........................................11
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1. Introduction
1.1. What is Nano-EHS?
Nano-EHS is a shorthand term for nanotechnology-related environmental, health, and
safety issues, which may determine the potential risks of engineered nanomaterials
(ENMs)1 and nanotechnology-enabled products (NEPs)2 to the environment and to
humans. Nanotechnology has already led to new and improved products and remains
poised to further “transform production processes and consumer products for everything
from traditionally high-tech products like computers to less obvious sources of
innovation and growth like sunscreen and paint” [1]. Potential nano-EHS risks must be
identified, assessed, and managed to enable widespread commercialization and adoption
of ENMs and NEPs. Knowledge of such risks to workers, the public, and the
environment will enable appropriate regulatory measures to be established, thus
alleviating consumer concerns and spurring development and manufacturing of ENMs
and NEPs. To perform science-based assessment and management of nano-EHS risks,
industry and regulatory agencies need access to and the means to generate accurate and
reproducible data on properties, exposure, and hazards of ENMs and NEPs.
1.2. The National Nanotechnology Initiative and Nano-EHS
The use of nanomaterials in art dates to the 4th century BC [2] and there are numerous
examples of nanotechnology innovations dating from the mid-to-late 1900’s, such as the
scanning tunneling microscope that enabled single atom imaging, the semiconductor
transistor that is the basis of integrated circuits, and the discovery of novel nanomaterials
including carbon nanotubes and quantum dots. In 2000, President Clinton launched the
National Nanotechnology Initiative (NNI) to coordinate Federal agency nanotechnology
efforts and to spur U.S competitiveness in nanotechnology, which led to the rapid
promulgation of the term ‘nanotechnology’. Three years later, Congress enacted the 21st
Century Nanotechnology Research and Development Act [3], which established the
statutory foundation for the NNI. The first NNI Strategic Plan [4], written by NNI
Federal agency representatives to the Nanoscale Science, Engineering, and Technology
Subcommittee (NSET) of the National Science and Technology Council’s Committee on
Technology, was published in 2004. One of the Plan’s four goals was to Support the
Responsible Development of Nanotechnology, which largely concerned nano-EHS issues.
In addition, the formation of a Nanotechnology Environmental and Health Implications
(NEHI) Working Group consisting of Federal agency representatives was mandated in
this Strategic Plan. The criticality of addressing EHS issues led to the 2006 publication
of a document addressing nano-EHS research needs [5]. Subsequently, strategies for
nano-EHS research in the Federal government were published in 2008 [6] and 2011 [7].
The NEHI Working Group developed all three of these documents, and NIST staff
members have played an active and leading role in the NEHI Working Group since its
inception. In addition, NIST led the development of a 2014 report [8] documenting the
1 Engineered nanomaterials (ENMs) are materials that have been purposely synthesized or manufactured to
have at least one external dimension of approximately 1 to 100 nanometers (nm)—at the nanoscale—and
that exhibit unique properties determined by this size. [7] 2 Nanotechnology-enabled products (NEPs) are intermediate engineered nanoscale products, including
ENMs embedded in a matrix material, that exist during manufacture and in final products. [7]
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accomplishments and coordination of the NNI-NEHI agencies in response to the needs
called out in the 2011 strategy document.
1.3. The NIST Role in Federal Nano-EHS Efforts
Figure 1 illustrates the inter-relationships and synergies of the six core research
categories in the 2011 nano-EHS research strategy. The
product of exposure and hazard is a measure of the risks
of ENMs to humans and the environment. Quantifying
risk requires accurate and reproducible measurements,
which are central to the Nanomaterial Measurement
Infrastructure (NMI) research category. The NMI
consists of a “suite of complementary tools for accurate,
precise, and reproducible measurements [that] is critical
for reliable assessment of exposure and hazards for
humans and the environment across all life cycle stages
of…ENMs and…NEPs” [1]. The NMI is foundational
because of the role “measurement tools play in supporting
and enabling the research needs in the other research
categories” [1]. Measurement tools are defined as methods,
protocols, standards (reference material and documentary),
instruments, models, and benchmark (validated) data. The goals of the NMI core research
area are two-fold:
(1) Develop measurement tools to detect and identify engineered nanoscale materials
in products and relevant matrices and determine their physico-chemical properties
throughout all stages of their life cycles
(2) Develop measurement tools for determination of biological response, and to
enable assessment of hazards and exposure for humans and the environment from
ENMs and NEPs throughout all stages of their life cycles.
NIST is the lead agency for the NMI research category. As described in subsequent
sections of this report, the NIST Nano-EHS Program was well-aligned with the NMI
goals.
2. History of the NIST Nano-EHS Program
2.1. Biomedical Applications
Four years prior to the establishment of the NIST Nano-EHS Program, a NIST-wide
effort in nanomaterial metrology and standards was initiated, with a focus on
nanoparticles for cancer therapeutics. In 2005, the National Cancer Institute (NCI)
established the Nanotechnology Characterization Laboratory (NCL) [9], the activities of
which represent a formal scientific partnership between the NCI, the Food and Drug
Administration (FDA), and NIST. The NCL’s mission is to “perform and standardize the
pre-clinical characterization of nanomaterials intended for cancer therapeutics and
diagnostics…and facilitate the development and translation of nanoscale particles and
devices for clinical applications” [9]. The NCI awarded NIST $1.0 M/y for three years to
develop quantitative, reproducible measurement methods and protocols for nanoparticle
Fig 1. Interrelationships of
the six core research areas
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characterization and to collaborate with NCI and FDA researchers to determine the best
measurement tools, protocols, and analysis methods for physically characterizing
nanoparticles. One key output of the partnership was the production of three gold
nanoparticle reference materials (RMs) with nominal diameters of 10 nm [10], 30 nm
[11], and 60 nm [12]. These nanoscale RMs, formally requested by the Office of the
Director of NCI, were the first of their kind appropriate for biomedical-related studies
and applications. As a direct result of the gold nanoparticle RM project, NIST gained
critical expertise and established core capabilities across a broad range of ENM property
measurements, including quantitative analysis of nanomaterial size using six independent
measurement techniques. This expertise and associated capabilities provided the initial
foundation on which the NIST Nano-EHS Program was built, and established NIST
internationally as a leader in nanomaterial metrology.
2.2. Nano-EHS Funding
Formal NIST-wide programs are typically established with new, federally appropriated
“Initiative” funds that are designated for a specific topic. Such funds are a common
means of increasing the NIST Scientific and Technical Research and Services (STRS)
budget. After five years, Initiative funds become general undesignated STRS funds. The
Program received funds from two Initiatives: Nano-EHS in 2009 and Nanomanufacturing
in 2012. Additional one-year funds were received from the NIST Director in 2010 and
2011. These designated funds are summarized in Table 1. Many of the Divisions
involved in the Program supplemented their nano-EHS activities with their own STRS
funds; these funds are not included in Table 1.
Table 2. Nano-EHS investments reported to the NNI
Funds by Fiscal Year, $ M
Source of Funds 2009 2010 2011 2012 2013 2014 2015 2016
Nano-EHS Initiative 1.8 1.8 1.8 1.8 1.8
NIST Director 1.0 1.0
Nanomanufacturing
Initiative 2.0 2.0 2.0 2.0 2.0
Total funds 1.8 2.8 2.8 3.8 3.8 2.0 2.0 2.0
Investments by Fiscal Year, $ M
2009 2010 2011 2012 2013 2014 2015 2016
3.5 3.4 3.2 7.2 6.2 5.1 6.7 5.9
Table 1. Designated Nano-EHS funds
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Annually, each Federal agency participating in the NNI is required to report its
investments by topic, known as Principal Component Areas (PCAs). These investments
are included in the annual NNI Supplement to the President’s Budget; the figures that
NIST reported for the EHS PCA for years 2009-2016 [13-20] are shown in Table 2. The
funding levels in Table 2 were obtained by directly querying the NIST Operating Units
and include both designated and division funds.
2.3. Nano-EHS Program Researchers
Since its inception in 2009, the nano-EHS Program has involved researchers from at least
seven Divisions and three Laboratories (Operating Units) within NIST. From 2012-2016,
the participating Labs and Divisions were:
Engineering Laboratory
Materials and Structural Systems Division, 731
Material Measurement Laboratory
Materials Science and Engineering Division, 642
Materials Measurement Science Division, 643
Biosystems and Biomaterials Division, 644
Chemical Sciences Division, 646
Applied Chemicals and Materials Division, 647
Physical Measurement Laboratory
Engineering Physics Division, 682
More than 90 researchers have worked on the Program over its eight-year span. The
researchers, listed in Appendix A, are grouped into five categories: (1) NIST principal
investigators; (2) NIST contributing staff members; (3) NRC postdoctoral fellows; (4)
Postdoctoral research associates; and (5) Student research associates.
3. NIST Nano-EHS Program Goals and Projects
Throughout the tenure of the Program, the overarching focus has been on the
development of measurement tools, defined here as methods, instrumentation, protocols
and assays, and RMs. In developing measurement tools, studies on specific ENMs
produced validated data that were published. The term “validated” implies that the data
were reproducible and generated by metrologically valid methods to ensure the greatest
accuracy and “quality” of the data.
From the outset, the Program focused on ENMs of greatest regulatory concern based on
production volume, widespread use in NEPs, and likely hazards—namely, silver (Ag)
and titanium dioxide (TiO2) nanoparticles, and carbon nanotubes (CNTs), both single-
wall (SW) and multi-wall (MW). Gold (Au) nanoparticles are a key benchmark material
for physico-chemical and toxicological measurements and are important in advanced
biomedical applications such as cancer treatment. As the Program progressed, the media
in which measurements were performed transitioned from simple media (e.g., air,
vacuum, water) to complex media, including both environmental (e.g., sediment, soil)
and biological (e.g., blood, tissue) media. From 2012–2016, a portion of the Program was
devoted to the application of measurement tools to specific ENM-NEP systems.
Throughout the Program, many researchers led or contributed to the development of
documentary standards and guidance documents in three standards-related organizations,
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namely ASTM International, the Organization for Economic Cooperation and
Development (OECD), and the Organization for International Standardization (ISO).
3.1. 2009‒2011
In 2009, a Steering Committee was formed whose function was to distribute the Nano-
EHS Initiative and NIST Director’s funds. In 2009 and 2010, the funds were used to
support single principal investigator research activities on the order of $25 K‒$150 K.
These activities focused on the development of methods to measure physico-chemical
and biological properties of ENMs and on the development of ENM RMs. Examples of
activities included the development of single-wall carbon nanotube and titanium dioxide
RMs, methods for stabilizing silver nanoparticles in environmental and biological media,
and protocols for assessing DNA damage in plants and organisms due to the presence of
ENMs. These activities were not centrally coordinated, though some involved informal
interactions between researchers at NIST and researchers from other government
agencies, industry, and academia.
In 2011, the Steering Committee defined three Program focus areas: (1) the determination
of surface attributes and transformations involving molecular adsorbents on ENM
surfaces; (2) measurement of the concentrations of nano-silver and silver ions in various
media; and (3) toxicological measurements. Although the activities within the focus areas
were not centrally coordinated, the collaborations among NIST staff members increased
substantially and channels for information sharing became well established.
3.2. 2012‒2014
Beginning with the award of the Nanomanufacturing Initiative in 2012, a Technical
Program Director was appointed to coordinate the Nano-EHS Program and the Steering
Committee was disbanded. Three-year (2102‒2014) Program and Spend Plans were
developed by this Director and approved by the NIST Director’s Office. The Plans were
closely aligned with the research needs in the Nanomaterial Measurement Infrastructure
(NMI) research category of the 2011 Nano-EHS Research Strategy [1]. Coordination
with other NNI-NEHI agencies was strengthened and collaborations among various
agencies were initiated and expanded, some continuing through 2016. Funds were
allocated for specified research activities by designated researchers in the Divisions. The
goals of the Program were two-fold:
(1) Enable other organizations to perform accurate and reproducible measurements
by providing validated measurement tools
(2) Enable other organizations to detect and quantitatively characterize ENMs in
NEPs using broadly available, commercial instruments
Specific deliverables by year for 2012-2014 are presented in the Program Plan document
in Appendix B.
3.2.1. Goal 1
There is an endless combination of ENMs subjected to various media during their
lifecycles; thus, it was clear that NIST could not determine the properties of all ENMs of
interest to multiple stakeholder groups under all possible scenarios. To maximize the
impact of its investment, NIST focused on the provision of measurement tools to enable
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other organizations to perform reproducible and accurate measurements on their own
materials. This necessitated that the Program focus, to the extent possible, on common,
affordable, and widely used instruments for which access was readily available to many
organizations.
The objectives of Goal 1 were to conduct the following activities of high-priority as
determined by interactions with NNI-NEHI agency and industrial representatives:
a) Develop and release RMs
b) Develop and broadly disseminate validated measurement methods and protocols
c) Lead and provide strong technical contributions to documentary and pre-
documentary standards development activities
3.2.2 Goal 2
For the duration of the Program, the number of NEPs on the market has continually
increased [21]. Two prevalent NEPs are fabrics (textiles) containing nano-scale Ag, and
NEPs manufactured from MWCNT-polymer composites. These two NEPs are the focus
of the two objectives for Goal 2:
a) Develop methods to detect and quantitatively characterize key properties3 of
Ag nanoparticles in fabrics
b) Develop methods to detect and quantitatively characterize key properties4 of
MWCNTs in polymer matrix-based NEPs
Teams were established among NIST Program participants to address the objectives for
Goals 1 and 2. Team members also worked closely with other key agency partners,
notably two of the five US regulatory agencies, i.e., the Consumer Product Safety
Commission (CPSC) and the FDA, as well as other National Metrology Institutes
(NMIs), including NRC Canada and BAM in Germany, and the European Commission
Institute for Reference Materials and Methods (now the Joint Research Centre).
3.3. 2015‒2016
In 2015, four new project areas were defined by the Program Director in collaboration
with several principal investigators in the Program. Funds were distributed to the seven
participating Divisions for specific activities in these new projects and in an overarching
measurement tool project that is a continuation of the work in Goal 1 above. These
projects continued through 2016, when the NIST Nano-EHS Program formally ended.
The five project areas were:
1) Measurement Tools
2) Release of MWCNTs from Polymer Composites
3) Graphene in Microelectronic Devices
4) Engineered Nanomaterials in Heterogeneous Matrices
5) Lifecycle Speciation of Nano-silver
3 For example, number concentration and size and size distribution of Ag NPs; distribution and chemical
form of Ag in fabrics. 4 For example, size and size distribution, morphology, and number concentration of MWCNTs; distribution
of MWCNTs in matrix.
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Plans for each project were developed that included a team leader, team members, project
goal, objectives, and deliverables by objective.
4. NIST Nano-EHS Program Outputs
During its eight-year tenure, the NIST Nano-EHS Program was prolific by any objective
measure, producing a substantial number of publications, protocols, and RMs. Each
output type will be described separately below.
4.1. Publications
The publications associated with the Program, presented in Appendix C, are organized by
type and year published (2009-2018). The type and total number of each are as follows:
1) Archival journal publications: 212
2) Conference proceedings: 25
3) NIST Technical Notes: 3
4) Book chapters: 14
In addition, two team members are co-editors of
the book Metrology and Standardization of
Nanomaterials - Protocols and Industrial
Innovations, which has 31 chapters.
One commonly used metric of a publication’s
impact is the Journal Impact Factor (JIF). JIF is a
measure that reflects the yearly average number of
citations to recent articles published in
that journal. 126 of the 212 archival journal publications had JIF values greater than 3.
Table 3 shows the number of publications for several ranges of JIF values. JIF values of 5
or above are generally considered representative of “high impact” journals.
The journals with the greatest number of publications are:
• Analytical and Bioanalytical Chemistry: 23
• Environmental Science and Technology: 21
• Journal of Nanoparticle Research:13
• ACS Nano: 11
• Nanotoxicology: 9
These journals demonstrate the breadth of the NIST Nano-EHS Program, encompassing
physico-chemical, environmental, and toxicological measurement research. As noted in
Appendix C, several articles received special recognition from the journals in which they
were published.
4.2. Protocols and Assays
Protocols and assays, defined here as step-by-step, reproducible, and validated
procedures (methods), are an essential first step in the harmonization of ENM/NEP
property measurements by enabling direct comparisons of data between laboratories and
greater consistency in reporting data. Protocols may address, either separately or
JIF range Number of
publications
3-5 46
5-10 63
10-15 17
Table 3. Number of publications
per JIF range.
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conjointly, sample preparation, conduct of measurements, and data analysis. The need for
and importance of protocols are called out in the 2011 Nano-EHS Research Strategy [1],
by agencies that regulate ENMs and NEPs, and by industry. Protocols can form the basis
for the development of documentary standards published by ISO, ASTM International,
and other standards-related organizations.
The list of nanomaterial measurement protocols and assays relevant to nano-EHS that
NIST published from 2012–2018 is presented in Appendix D. NIST has a dedicated web
site containing 24 publicly available nanomaterial measurement protocols; see
https://www.nist.gov/mml/nano-measurement-protocols. These protocols have been
published in the 1200 series of NIST Special Publications (SPs) with citable DOI names
to provide persistent identification. Five of these protocols were developed in conjunction
with the Center for the Environmental Implications of NanoTechnology, a multi-
university entity led by Duke University with funding from the National Science
Foundation and the Environmental Protection Agency. In addition, NIST team members
have led the development of 11 assays that are publicly available on NCL’s Assay
Cascade Protocol web site https://ncl.cancer.gov/resources/assay-cascade-protocols.
4.3. Reference Materials
Reference materials (RMs) is a generic term used here to include NIST Reference
Materials, NIST Traceable Reference Materials™ and NIST Standard Reference
Materials™ [22]. Definitions of these three types of RMs are provided on the NIST web
site [23].
The RMs of relevance to the Nano-EHS Program are listed in Appendix E, which
includes technical and sales information. As mentioned previously, the NIST Nano-EHS
Program focused on ENMs of greatest regulatory concern based on production volume,
widespread use in NEPs, and potential hazards—namely, silver (Ag) and titanium
dioxide (TiO2) nanoparticles and carbon nanotubes (CNTs), both single-wall (SW) and
multi-wall (MW). From 2011-2018, NIST produced RMs for each of these ENMs. The
three gold nanoparticle RMs, though released in 2008, are included in Appendix E
because the large majority of the sales of these RMs occurred post-2008. To date, more
than 2050 units of the nine RMs listed in Appendix E have been delivered to stakeholders
world-wide.
4.4. Documentary Standards
ISO Technical Committee (TC) 229 on Nanotechnologies and ASTM International
Committee E56 on Nanotechnology are arguably the two prevalent standards
development organizations (SDOs) in nanotechnology. NIST researchers have played
prominent leadership roles in these SDOs, both at the committee level and for specific
technical standards.
Committee-level leadership positions include:
• Chair, US Technical Advisory Group (TAG) to ISO TC229 (2005–2010 and
2015–2016)
• Chair, US TAG to ISO TC229 Joint Working Group 2 (JWG2). Measurement and
Characterization (2005–2016)
• Convener, ISO TC229 WG 3, Health, Safety and the Environment (2006–2013)
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• Chair, ASTM Committee E56 (2009–2015)
• Vice-Chair, ASTM Committee E56 (2015–2016)
• Co-Chair, ASTM Subcommittee E56.02, Physical and Chemical Characterization
(2015–2016)
• Chair, ASTM Subcommittee E56.05, Liaison and International Cooperation
(2012–2016)
• Chair, ASTM Subcommittee E56.07, Education and Workforce Development
(2014–2016)
NIST researchers have also led or co-led the writing nearly 20 ISO and ASTM standards,
including those currently under development. NIST researchers have also participated
substantially in the development of other standards as approved experts serving on the
US delegation to ISO 229 and as subject matter experts within ASTM E56. Another
international effort in which NIST researchers have been involved is the Organization for
Economic Co-operation and Development (OECD), which has produced guidelines
pertinent to nano-EHS.
5. NIST Nano-EHS Program Impacts
The number, quality, and breadth of outputs are indicative of the significant impacts of
the NIST Nano-EHS Program. Two case studies presented below illustrate the magnitude
of specific impacts.
5.1. Case Study I: Gold Nanoparticle Reference Materials
In 2008, NIST released a series of three gold nanoparticle
RMs: 8011, nominal diameter = 10 nm; 8012, nominal
diameter = 30 nm; and 8013, nominal diameter = 60 nm (Fig.
2). Nanoparticle sizes were determined by six independent
techniques, five of which use commonly available
commercial instruments. While the RMs were originally
intended to support pre-clinical biomedical efforts, they have
found great utility in nano-EHS research and metrology
development. Though anticipated to be used primarily to
evaluate and qualify methodology and instrument
performance for dimensional measurements, the RMs have
been employed to develop and evaluate in vitro assays
designed to assess biological response (e.g., cytotoxicity and
hemolysis) of ENMs. Further, the RMs have been used in
interlaboratory test comparisons for the development or uncertainty analysis of three
ASTM E56 and one ISO TC 229 standard. RMs 8012 and 8013 have been widely
adopted as calibration standards for single particle inductively coupled plasma mass
spectrometry, an important and rapidly emerging measurement technology. Collectively
and as of April 2018, 1783 units of the gold RMs have been sold in nearly equal numbers
to US and foreign organizations.
Fig. 2. Units of RMs
8011, 8012, and 8013. ______________________________________________________________________________________________________
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A detailed impact study was performed on RM 8012 [11], with information collected and
analyzed as of July 10, 2015. Sales statistics for RM 8012 are presented in Table 4. It is
notable that, of the 479 units sold, nearly 90 % were purchased by industry and
government agencies, including National
Metrology Institutes world-wide.
As of August 2016, there were more than
90 peer-reviewed publications and 8 non-peer
reviewed documents (application notes,
documentary standards, white papers, and
notes) that utilize one or more of the three
gold RMs (8011, 8012, and 8013) for a
variety of purposes, or in which the gold RMs
are a significant focus of discussion. A graph
of the publications related to the gold RMs as
of September 2015 is shown in Fig. 3. The
principal uses of the gold RMs, from both
published and anecdotal sources, include:
• Quality control and quality assurance
(especially in analytical services labs and
pharmaceutical companies)
• Method and instrument calibration
• Interlaboratory studies and comparisons
• Basic research
• Metrology research
• Method and technique comparisons
• Toxicological and environmental
investigations
In summary, the NIST gold nanoparticle RMs have been used across the world, with
significant impacts on nano-EHS, biomedical applications and nanometrology as
demonstrated by sales and documented uses.
5.2. Case Study II: Measurement Assurance for a Nanotoxicity Assay
Cell-based toxicity assays (i.e., cytotoxicity assays) are commonly employed as screening
tools to identify potential hazards associated with new chemicals and materials used in
manufacturing. These assays are also used to evaluate biological effects associated with
ENMs. Significant variability in such assays due to various sources have led to
conflicting hazard data. For ENMs, some sources may include nanometer dimensions,
large surface-to-volume ratios, wide ranges of composition and coatings, and the
introduction of ENMs into living cell culture systems. The need to improve cell-based
assays for nano-cytotoxicity has been demonstrated in interlaboratory studies coordinated
by the International Alliance for Nano-EHS Harmonization wherein large variabilities in
measurements were obtained.
Purchasers of RM 8012 Units, number or
% of total sold
Total number 479
Domestic organizations 47%
Foreign organizations 53%
Industry 46%
Government 42%
Academia 12%
NMIs (part of government) 12 Publications Related to NIST Gold RMs
year
2007 2008 2009 2010 2011 2012 2013 2014 2015
nu
mb
er
of
pu
blic
atio
ns
0
5
10
15
20
25
30
non-peer reviewed
peer reviewed
rele
ase o
f R
Ms
total publications = 93
Fig 3. Number of publications by year.
Table 4. Purchasers of RM 8012 as of September 2015
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In response to this need, researchers in the Cell Systems Science group developed an
approach to determine sources of variability that uses a novel measurement system to
assess quality metrics for nano-cytotoxicity assay performance. The system is a 96-well
plate based on the well-known MTS assay and uses protocols for cell line identification
testing, dosing preparation, and pipetting procedures. Seven in-line quality assessment
controls include reagent quality, cell seeding quality, cell function, and nanoparticle
interference (Fig. 4). Measurements using the well plate and associated protocols yield a
nano-cytotoxicity value and six additional results that characterize the measurement
system. The system enables intermediate measurements pertinent to the assay that could
be used to validate comparability of measurements between different laboratories and
different nanomaterials.
The validity of the measurement system was assessed by an interlaboratory study
including EMPA (Switzerland), NanoTEC (Thailand), Joint Research Centre (European
Commission) and KRISS (Korea). The results of this study indicated several sources of
variability associated with: (1) cell line identification; (2) rinsing attached cell layers; and
(3) nanoparticle dispersion techniques. The large number of data sets from the different
laboratories resulted in performance specifications for each of the in-line process controls
and provided criteria that can be used to ensure comparability between data sets.
This work culminated in three publications [24-26] and the development of an ISO
International standard (ISO/DIS 19007: Nanotechnologies – In vitro MTS assay for
measuring the cytotoxic effect of nanoparticles) using the MTS assay in nano-
cytotoxicity testing [14-16]. This work serves as an exemplar for developing high-
quality assays and translating measurement science into a documentary standard.
Fig. 4. 96-well plate layout for cytotoxicity assays on ENMs
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6. Conclusions
The eight-year NIST Nano-EHS Program has been successful by several objective
measures. Outputs from the Program—publications, protocols, and RMs—are diverse
and large in number. The significant impact of the Program has been demonstrated here
through two case studies: the NIST gold nanoparticle RMs and the toxicity assay
measurement assurance. Beginning in 2012, the teamwork demonstrated by all the
researchers has been profound. The measurement infrastructure and knowledge base
established through the NIST Nano-EHS Program will be beneficial in other innovative
application areas of importance to commerce and healthcare, such as biomedical devices,
energy generation, and water purification. The combined experience, expertise, and
facilities resulting principally from the Program represent new core competencies at
NIST, which can be further exploited to address a wide range of nanotechnology
measurement issues of importance to a broad range of stakeholders, including industry
and regulatory bodies. Finally, the interdivisional and interdisciplinary network of
scientists, established in large part due to the Program, will have a lasting legacy that
reaches beyond nano-EHS and nanotechnology.
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Acknowledgements
The authors would like to thank John Elliott and Elijah Petersen of NIST for contributing
Case Study II: Measurement Assurance for a Nanotoxicity Assay.
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[24] Rosslein M, et al. (2015) The use of cause-and-effect analysis to design a high-
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https://doi.org/10.1021/tx500327y
[25] Toman B, Rosslein M, Elliott J, Petersen EJ (2016) Estimation and uncertainty
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[26] Elliott JT, et al. (2017) Toward achieving harmonization in a nano-cytotoxicity assay
measurement through an interlaboratory comparison study. Altex 34(2):201-218.
https://doi.org/10.14573/altex.1605021
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*the researcher is no longer at NIST
Appendix A: Nano-EHS Program Researchers
(most recent position held)
NIST Staff: Principal Investigators
John Elliott
Jeffrey Fagan
Jeffrey Gilman
Justin Gorham
Vincent Hackley
Angela Hight-Walker
R. David Holbrook
Robert MacCuspie*
Elisabeth Mansfield
Karen Murphy
Bryant Nelson
Elijah Petersen
John Pettibone
Vytas Reipa
Keana Scott
LiPiin Sung
Andras Vlàdàr
Michael Winchester
NIST Staff: Contributing Members
Donald Atha
T. J. Cho
Miral Dizdaroglu
Shannon Hanna*
Deborah Stanley Jacobs
Pawel Jaruga
Monique Johnson
Peter Krommenhoek*
Stephen Long
Rabia Oflaz
Alex Peterson
Savelas Rabb
Marc Salit
Blaza Toman
Wyatt Vreeland
Stephanie Watson
Jeremiah Woodcock
Lee Yu
Rolf Zeisler
Justin Zook
NRC Postdoctoral Fellows
Mark Bailey
Michelle Blickley
Christopher Brown
Danielle Cleveland
Chelsea Davis
Sherrie Elzey
John Heddleston
Constantine Khripin
Stephanie Lam
Christian Long
Stacey Louie
Bryce Marquis
Grant Myers
Nathan Orloff
Fatima Sequeira
Christopher Sims
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NIST Associates: Post-docs
Jens Breffke
Bryan Calderon Jimenez
Ning Chen
Guangun Cheng
Hsiang Chun Hsueh
Hind El Hadri
Julien Gigault
Preshagar Kavuri
Sung Kim
Thomas Lam
Jingyu Liu
Arnab Mukherjee
Antonio R. Montoro Bustos
Bharath Natarajan
Liz Nguyen
Tinh Nguyen
Yongyan Pang
Yanmei Piao
Vinayak Rastogi
Carlos Silvera Batista
Julian Taurozzi
Vipin Tondare
De-Hao Tsai
Ji Yeon Huh
Minhua Zhao
NIST Associates: Students
George Caceres
Yu-Lun Cheng
Yu-Fang Chuang
Anne Galyean
Carly Geronimo
James Ging
Sin-Ru Huang
Samuel Norris
Bastien Pellegrin
Cristina Rios Valdez
Brian Stock
Jiaojie Tan
Chun-Chieh Tien
Chen-Hsiang Tsai
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Appendix B: Nano-EHS Initiative Program Plan, FY12-14
Excerpts from the Program Plan are given below.
Program Goals, Objectives, and Deliverables
The technical work described below will significantly advance the establishment of a
nanomaterial measurement infrastructure consisting of critical tools—standards,
measurement methods, and validated data and models. The technical scope of the work
will encompass four of the five Research Needs identified in the Nanomaterial
Measurement Infrastructure Research Chapter of the NNI 2011 Nano-EHS Research
Strategy: (1) determination of the physico-chemical properties of ENMs, a necessary first
step in exposure and hazard evaluation; (2) detection of ENMs and NEPs; (3) evaluation
of transformations of ENMs; and (4) evaluation of biological responses to ENMs and
NEPs. The Program will provide the metrological foundation and measurement tools
essential to the fifth Research Need, evaluation of release mechanisms of ENMs from
NEPs. To maximize the relevance and impact of NIST work, FY12-FY14 priorities in
Research Needs (1) and (2) are MWNCTs in polymer matrix-based NEPs such as
sporting goods, and Ag NPs in NEPs such as fabrics. These ENM-NEP priorities are also
consistent with those of the NanoRelease Project, a group of international representatives
and technical experts from government agencies, industry, non-governmental
organizations, and universities focused on the identification and development of methods
to detect and characterize ENMs released from NEPs.
A. Objective: Develop and release standard reference materials (SRMs) and
reference materials (RMs)
Task FY Deliverable
i
Develop methods for next-
generation SRMs and RMs, i.e.,
zeta potential measurement,
positive toxicity controls
12 Progress reports
ii
Complete SRMs and RMs for key
ENMs (TiO2 and Ag NPs and
single-wall CNTs) certified for
specific surface area and
dimensions
12 SRMs and RMs
iii
Demonstrate the applicability of
new hyphenated instruments to
next generation SRMs and RMs,
i.e., ENMs in complex matrices
and Ag NPs in aqueous media
12-
13 Progress reports
Goal 1: Enable other organizations to perform accurate, precise, and reproducible
measurements by providing measurement tools
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iv
Design and produce prototype
SRMs and RMs for zeta potential
measurement and positive
toxicity controls
12-
13
Progress reports,
prototype SRMs and
RMs
v
Design and produce prototype
SRMs and RMs for determination
of chirality in purified SWCNTs
12-
13
Progress reports,
SRMs and RMs
vi
Develop methods and produce
prototype SRMs and RMs for
ENMs in complex matrices such
as soil
13-
14
Progress reports,
prototype SRMs and
RMs
vii
Develop methods and produce
prototype SRMs and RMs for
determination of concentration of
total Ag, Ag ions, and Ag NPs in
relevant media
13-
14
Progress reports,
prototype SRMs and
RMs
viii
Evaluate potential for RMs on
other key ENMs, i.e., MWCNTs,
CeO NPs, and nanoclays
13-
14 Progress reports
ix
Initiate production of SRMs and
RMs for zeta potential
measurement, positive toxicity
controls, and determination of
chirality in purified SWCNTs
14 WCF proposals,
progress reports
B. Objective: Develop and broadly disseminate validated measurement
protocols and assays
Task FY Deliverable
i
Prepare manuscripts on three
NIST protocols for dispersion of
TiO2 in various media
12
NIST Special
Publications (SPs)
NIST website postings
ii
Demonstrate the adequacy and
extensibility of at least two
existing in vitro and in vivo
toxicity assays to ENMs
12 Progress reports,
publications
iii
Complete a VAMAS
interlaboratory study (ILS) on
chirality measurements of single
wall CNT mixtures and develop
a protocol
12-
13
Report on ILS results
NIST SP on protocol
NIST website posting
iv Develop protocols to stabilize
soluble NPs such as Ag
12-
13
NIST Special
Publication (SP)
NIST website posting
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v
Develop in vitro and in vivo
toxicity assays, based on
existing or new assays
13-
14
Progress reports,
publications
vi
Evaluate and initiate
development of sample
preparation and measurement
protocols for other key ENMs,
i.e., MWCNTs, and CeO NPs,
and nanoclays
13-
14
Reports by study
groups (internal and
external) and on ILS’s
initiated in VAMAS
and ASTM E56
vii
Develop draft protocols for the
use of hyphenated instruments,
e.g., DMA/AFFF/ICP-MS
14 Progress reports
C. Objective: Lead and provide strong technical contributions to
documentary and pre-documentary standards development activities
Task FY Deliverable
i
Increase staff leadership and
participation in nano-EHS-
related SDOs and pre-
standardization organizations
12-
14
Listing of leadership
positions and active
staff members
ii
i. Lead and participate in the
completion and publication of
ongoing work items
12-
13
Listing of published
standards with noted
NIST leadership role
iii Lead and participate in the
development of new work items
12-
14
Listing of new work
items with noted NIST
leadership role
Progress reports
iv
Co-organize workshops that
enable the prioritization and
increased use and value of
documentary standards
12-
14
Workshop reports
v
Facilitate communication,
cooperation, and coordination of
activities among SDOs
12-
14
Reports describing
actions taken
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A. Objective: Develop methods to detect and quantitatively characterize Ag
NPs in fabrics
Task FY Deliverable
i
Evaluate the applicability,
advantages, and limitations of
FE-SEM, TEM, AFM, ICP-MS,
SEC, and XPS for the detection
of Ag NPs; develop sample
preparation approaches for each
method
12
Progress reports,
publications
ii
Evaluate the applicability,
advantages, and limitations of
FE-SEM, TEM, AFM, ICP-MS,
SEC, and XPS for quantitative
measurements of Ag NPs;
identify specific properties that
can be determined with each
method
12-
13
Progress reports,
publications
iii
Generate data and associated
measurement uncertainties using
FE-SEM, TEM, AFM, ICP-MS,
SEC, and XPS
13-
14
Progress reports,
publications
iv
Evaluate the feasibility of
extending the capabilities of FE-
SEM, TEM, AFM, ICP-MS,
SEC, and XPS, (e.g., high
throughput and three-
dimensional measurements) for
the detection and
characterization of Ag NPs
14
Progress reports,
publications
Goal 2: Enable other organizations to detect and quantitatively characterize ENMs in
NEPs using broadly available, commercial instruments
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B. Objective: Develop methods to detect and quantitatively characterize
MWCNTs in polymer matrix-based NEPs
Task FY Deliverable
i
Evaluate the applicability,
advantages, and limitations of FE-
SEM, TEM, AFM, ICP-MS, SEC,
and XPS for the detection of
MWCNTs; develop sample
preparation approaches for each
method
12
Progress reports,
publications
ii
Evaluate the applicability,
advantages, and limitations of FE-
SEM, TEM, AFM, ICP-MS, SEC,
and XPS for quantitative
measurements of MWCNTs;
identify specific properties that
can be determined with each
method
12-
13
Progress reports,
publications
iii
Generate data and associated
measurement uncertainties using
FE-SEM, TEM, AFM, ICP-MS,
SEC, and XPS
13-
14
Progress reports,
publications
iv
Evaluate the feasibility of
extending the capabilities of FE-
SEM, TEM, AFM, ICP-MS, SEC,
and XPS, (e.g., high throughput
and three-dimensional
measurements) for the detection
and characterization of MWCNTs
14
Progress reports,
publications
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Appendix C: Nano-EHS Program Publications
(in increasing chronological order by type of publication)
Archival Journal Articles
1. Hackley VA, Fritts M, Kelly JF, Patri AK, Rawle AF (August 2009) Enabling
standards for nanomaterial characterization. InfoSim – Informative Bulletin of the
Interamerican Metrology System, The Organization of American States, 24-29.
2. Duan J, Park K, MacCuspie R, Vaia RA, Pachter R (2009) Optical properties of
rodlike metallic nanostructures: insight from theory and experiment. Journal of
Physical Chemistry C 113:15524–15532. https://doi.org/10.1021/jp902448f
3. Decker JE, et al. (2009) Sample preparation protocols for realization of
reproducible characterization of single-wall carbon nanotubes. Metrologia
46(6):682-692. https://doi.org/10.1088/0026-1394/46/6/011
4. Choi J, Wang NS, Reipa V (2009) Electrochemical reduction synthesis of
photoluminescent silicon nanocrystals. Langmuir 25(12):7097-7102.
https://doi.org/10.1021/la9001829
5. Choi J, et al. (2009) Comparison of cytotoxic and inflammatory responses of
photoluminescent silicon nanoparticles with silicon micron-sized particles in RAW
264.7 macrophages. Journal of Applied Toxicology 29(1):52-60.
https://doi.org/10.1002/jat.1382
6. Dobrovolskas D, Mickevicius J, Tamulaitis G, Reipa V (2009) Photoluminescence
of Si nanocrystals under selective excitation. Journal of Physics and Chemistry of
Solids 70(2):439-443. https://doi.org/10.1016/j.jpcs.2008.11.013
7. Zhou Z, et al. (2009) Water soluble DNA-wrapped single-walled carbon,
nanotube/quantum dot complexes. Small 5(19):2149–2155.
https://doi.org/10.1002/smll.200801932
8. Kang HG, et al. (2009) Multimodal, nanoscale, hyperspectral imaging demonstrated
on heterostructures of quantum dots and DNA-wrapped single-wall carbon
nanotubes. ACS Nano 3(11):3769-3775. https://doi.org/10.1021/nn901075j
9. Kang H, et al. (2009) Probing dynamic fluorescence properties of single and
clustered quantum dots towards quantitative biomedical imaging of cells. WIREs
Nanomedicine and Nanobiotechnology 2(1):48-58. https://doi.org/10.1002/wnan.62
10. Tyner KM, et al. (2009) Comparing methods for detecting and characterizing metal
oxide nanoparticles in unmodified commercial sunscreens. Nanomedicine 4(2):145-
159. https://doi.org/10.2217/17435889.4.2.145
11. Pease III LF, et al. (2009) Length distributions of single wall carbon nanotubes in
aqueous suspensions measured by electrospray-differential mobility analysis. Small
5(24):2894-2901. https://doi.org/10.1002/smll.200900928
12. Simpson JR, Fagan JA, Hobbie EK, Hight Walker AR (2009) The effect of
dispersant on defects in length-separated single wall carbon nanotubes measured by
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Raman spectroscopy. Carbon 47: 3238-3241.
https://doi.org/10.1016/j.carbon.2009.07.037
13. Xiao Y, et al. (2009) Anti-HER2 IgY antibody-functionalized single-walled carbon
nanotubes for detection and selective destruction of breast cancer cells. BMC
Cancer 9:351-1-11. https://doi.org/10.1186/1471-2407-9-351
14. Cho TJ, Hackley VA (2010) Fractionation and characterization of gold
nanoparticles in aqueous solution: asymmetric-flow field flow fractionation with
MALS, DLS, and UV–Vis detection. Analytical and Bioanalytical Chemistry
398:2003-2018. https://doi.org/10.1007/s00216-010-4133-6
15. Wu C, et al. (2010) Effect of nanoparticle clustering on the effective thermal
conductivity of concentrated silica colloids. Physical Review E 81:011406-1-7.
https://doi.org/10.1103/PhysRevE.81.011406
16. Dair BJ, et al. (2010). The effect of substrate material on silver nanoparticle
antimicrobial efficacy. Journal of Nanoscience and Nanotechnology 10:1-7.
https://doi.org/10.1166/jnn.2010.3566
17. Cleveland D, et al. (2010) Chromatographic methods for the quantification of free
and chelated gadolinium species in MRI contrast agent formulations. Analytical and
Bioanalytical Chemistry 398(7-8):2987-2995. https://doi.org/10.1007/s00216-010-
4226-2
18. Morrow JB, Arango C, Holbrook RD (2010) Association of quantum dot
nanoparticles with Pseudomonas aeruginosa biofilm. Journal of Environmental
Quality 39(6):1934-1941. https://doi.org/10.2134/jeq2009.0455
19. Holbrook RD, Kline CN, Filliben JJ (2010) Impact of source water quality on
multiwall carbon nanotube coagulation. Environmental Science & Technology
44(4):1386-1391. https://doi.org/10.1021/es902946j
20. Petersen EJ, Nelson BC (2010) Mechanisms and measurements of nanomaterial-
induced oxidative damage to DNA. Analytical and Bioanalytical Chemistry
398:613-650. https://doi.org/10.1007/s00216-010-3881-7
21. Reipa V, Purdum G, Choi J (2010) Measurement of nanoparticle concentration
using quartz crystal microgravimetry. Journal of Physical Chemistry B 49:16112-
16117. https://doi.org/10.1021/jp103861m
22. Huh JY, et al. (2010) Separation and characterization of double-wall carbon
nanotube subpopulations. Journal of Physical Chemistry C 114:11343-11351.
https://doi.org/10.1021/jp9110376
23. Mansfield E, Kar A, Hooker S (2010) Application of quartz crystal microbalances
at elevated temperatures as an alternative to TGA. Analytical Chemistry
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released from consumer products, NIST Technical Note 1787, 55 pp.
https://doi.org/10.6028/NIST.TN.1787
2. Persily A, Lo LC, Nabinger S, Poppendieck D, Sung L (2014) Characterization of
airborne nanoparticle released from consumer products. NIST Technical Note 1843,
36 pp. https://doi.org/10.6028/NIST.TN.1843
3. Sung L, Nguyen T, Persily A (2014) Nanoparticle released from consumer products:
flooring nanocoatings and interior nanopaints. NIST Technical Note 1835, 78 pp.
https://doi.org/10.6028/NIST.TN.1835
Book Chapters
1. Sung L, et al. (2009) Impact of nanoparticles on the scratch behavior of a
polyurethane coating. ACS Symposium Series 1008: Nanotechnology Applications in
Coatings, eds Fernando R, Sung L (ACS/Oxford University Press, Washington, DC),
Chapter 12, pp 232-254. https://doi.org/10.1021/bk-2009-1008.ch012
2. Watson S, Forster A, Tseng I, Sung L (2009) Assessment of spectrophotometric assay
methods on nanostructured pigments. ACS Symposium Series 1008: Nanotechnology
Applications in Coatings, eds Fernando R, Sung L (ACS/Oxford University, Press
Washington, DC), Chapter 17, pp. 349-372.
https://doi.org/10.1021/bk-2009-1008.ch017
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: https://doi.org/10.6028/NIS
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43
3. Galyean A, Weinberg HS, Holbrook D, Leopold M (2012) Characterization of
engineered nanoparticles in natural waters. Comprehensive Analytical Chemistry:
Analysis and Risk of Nanomaterials in Environmental and Food Samples, eds Barceló
D, Farré M (Elsevier, New York, NY), Vol. 59, pp 169-195.
https://doi.org/10.1016/B978-0-444-56328-6.00005-0
4. Nguyen T, Wohlleben W, Sung L (2014) Mechanisms of aging and release from
weathered nanocomposites. Safety of Nanomaterials Along Their Lifecycle: Release,
Exposure, and Human Hazards, eds Wohlleben W, Kuhlbusch TAJ, Schnekenburger
J, Lehr C-M (CRC Press, Boca Raton, FL), Chapter 14.
https://doi.org/10.1201/b17774-18
5. Petersen EJ (2014) Ecotoxicological effects of carbon nanotubes: methodological
issues and current research. Health and Environmental Safety of Nanomaterials, eds
Njuguna J, Pielichowski K, Zhu H (Woodhead Publishing, Cambridge, UK), pp 175-
199.
6. Holbrook RD, Galyean AA, Gorham JM, Herzing A, Pettibone J (2015) Overview of
nanomaterial characterization and metrology. Characterization of Nanomaterials in
Complex Environmental and Biological Media, eds Baalousha M, Lead JR (Elsevier,
Amsterdam, Netherlands), Chapter 2, pp 47-90.
https://doi.org/10.1016/B978-0-08-099948-7.00002-6
7. Mansfield E (2015) Recent advances in thermal analysis of nanoparticles: methods,
models and kinetics. Modeling, Characterization and Production of Nanomaterials:
Electronics, Photonics, and Energy Applications, eds Tewary VK, Zhang Y
(Woodhead Publishing, Cambridge, UK), Chapter 8, 1st Ed.,17 pp.
8. Johnston LJ, Mansfield E, Smallwood GJ (2017) Physicochemical properties of
engineered nanomaterials. Metrology and Standardization for Nanotechnology:
Protocols and Industrial Innovations, eds Mansfield E, Kaiser DL, Fujita D, Van de
Voorde M (Wiley-VCH Verlag GmBH & Co., Weinheim, Germany), pp 99-112.
https://doi.org/10.1002/9783527800308.ch5
9. Mansfield E, Hartshorn R, Atkinson A (2017) Nanomaterial recommendations from
the International Union of Pure and Applied Chemistry (IUPAC). Metrology and
Standardization for Nanotechnology: Protocols and Industrial Innovations, eds
Mansfield E, Kaiser DL, Fujita D, Van de Voorde M (Wiley-VCH Verlag GmBH &
Co., Weinheim, Germany), pp 299-305.
https://doi.org/10.1002/9783527800308.ch18
10. Kaiser DL (2017) Standards from ASTM International Technical Committee E56 on
Nanotechnology. Metrology and Standardization for Nanotechnology: Protocols and
Industrial Innovations, eds Mansfield E, Kaiser DL, Fujita D, Van de Voorde M
(Wiley-VCH Verlag GmBH & Co., Weinheim, Germany), pp 269-278.
https://doi.org/10.1002/9783527800308.ch15
11. Scott K, Pomar-Portillo V, Vázquez-Campos S (2017) Nanomaterials in textiles.
Metrology and Standardization for Nanotechnology: Protocols and Industrial
Innovations, eds Mansfield E, Kaiser DL, Fujita D, Van de Voorde M (Wiley-VCH
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: https://doi.org/10.6028/NIS
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44
Verlag GmBH & Co., Weinheim, Germany), pp 559-572.
https://doi.org/10.1002/9783527800308.ch31
12. Nelson BC, Reipa V (2017) Analytical measurements of nanoparticles in challenging
and complex environments. Metrology and Standardization for Nanotechnology:
Protocols and Industrial Innovations, eds Mansfield E, Kaiser DL, Fujita D, Van de
Voorde M (Wiley-VCH Verlag GmBH & Co., Weinheim, Germany), pp 115-127.
https://doi.org/10.1002/9783527800308.ch9
13. Roebben G, Hackley VA, Emons H (2017) Reference nanomaterials to improve the
reliability of nanoscale measurements. Metrology and Standardization for
Nanotechnology: Protocols and Industrial Innovations, eds Mansfield E, Kaiser DL,
Fujita D, Van de Voorde M (Wiley-VCH Verlag GmBH & Co., Weinheim,
Germany), pp 307-322. https://doi.org/10.1002/9783527800308.ch19
14. Chang C-H, Su P-J, Liu BH, Watson SS, Sung L (2017) Effect of UV radiation on
surface mechanical properties of nanoTiO2-acrylic urethane coatings. Service Life
Prediction for Polymers and Plastics Exposed to Outdoor Weathering, eds White CC,
White KM, Pickett JE (New York, NY, Elsevier), Chapter 14, pp 247-262.
Books Edited
1. Mansfield E, Kaiser DL, Fujita D, Van de Voorde M (2017) Metrology and
Standardization for Nanotechnology: Protocols and Industrial Innovations, (Wiley-
VCH Verlag GmBH & Co., Weinheim, Germany) 594 pp.
______________________________________________________________________________________________________ This publication is available free of charge from
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Appendix D: Nano-EHS Program Protocols and Assays
NIST Nano–Measurement Protocols
https://www.nist.gov/mml/nano-measurement-protocols
1. Taurozzi JS, Hackley VA, Wiesner MR (2012) Reporting guidelines for the
preparation of aqueous nanoparticle dispersions from dry materials. NIST Special
Publication 1200-1. Ver 2.1, 9 pp. http://dx.doi.org/10.6028/NIST.SP.1200-1
2. Taurozzi JS, Hackley VA, Wiesner MR (2012) Preparation of nanoparticle
dispersions from powdered material using ultrasonic disruption. NIST Special
Publication 1200-2. Ver 1.1, 15 pp. http://dx.doi.org/10.6028/NIST.SP.1200-2
3. Taurozzi JS, Hackley VA, Wiesner MR (2012) Preparation of a nanoscale TiO2
aqueous dispersion for toxicological or environmental testing. NIST Special
Publication 1200-3. Ver 1.2, 11 pp. http://dx.doi.org/10.6028/NIST.SP.1200-3
4. Taurozzi JS, Hackley VA, Wiesner MR (2012) Preparation of nanoscale TiO2
dispersions in biological test media for toxicological assessment. NIST Special
Publication 1200-4. Ver 1.1, 13 pp. http://dx.doi.org/10.6028/NIST.SP.1200-4
5. Taurozzi JS, Hackley VA, Wiesner MR (2012) Preparation of nanoscale TiO2
dispersions in an environmental matrix for eco-toxicological assessment. NIST
Special Publication 1200-5r1. Ver 1.2, 12 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-5r1
6. Hackley VA, Clogston JD (2015) Measuring the size of nanoparticles in aqueous
media using batch-mode dynamic light scattering. NIST Special Publication 1200-6.
Ver 1.2, 14 pp. http://dx.doi.org/10.6028/NIST.SP.1200-6
7. Gorham JM, et al. (2015) Preparation of silver nanoparticle loaded cotton threads to
facilitate measurement development for textile applications. NIST Special Publication
1200-8. Ver 1.0, 18 pp. http://dx.doi.org/10.6028/NIST.SP.1200-8
8. Davis CS, Woodcock JW, Gilman JW (2015) Preparation of multi-walled carbon
nanotube dispersions in a polyetheramine epoxy for eco-toxicological assessment.
NIST Special Publication 1200-9. Ver 1.0, 13 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-9
9. Gorham JM, Woodcock JW, Scott KC (2015) Challenges, strategies and
opportunities for measuring carbon nanotubes within a polymer composite by X-ray
photoelectron spectroscopy. NIST Special Publication 1200-10. Ver 1.0, 9 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-10
10. Petersen EJ (2015) Control experiments to avoid artifacts and misinterpretations in
nanoecotoxicology testing. NIST Special Publication 1200-11. Ver 1.0, 7 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-11
11. Reipa V (2015) Reconstitution of 2 nm diameter Silicon Nanoparticles (RM8027)
into aqueous solvents. NIST Special Publication 1200-12. Ver 1.0, 18 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-12
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12. Zook J, MacCuspie, R, Long SE, Petersen EJ (2015) Measurement of silver
nanoparticle dissolution in complex biological and environmental matrices using
UV/visible absorbance measurements. NIST Special Publication 1200-13. Ver 1.0, 6
pp. http://dx.doi.org/10.6028/NIST.SP.1200-13
13. Zook JM, MacCuspie RI, Elliott JT, Petersen EJ (2015) Reliable preparation of
nanoparticle agglomerates of different sizes in cell culture media. NIST Special
Publication 1200-14. Ver 1.0, 7 pp. http://dx.doi.org/10.6028/NIST.SP.1200-14
14. Sung L, Nguyen T (2015) Protocols for accelerating laboratory weathering and
measurements of degradation of polymer-multiwalled carbon nanotube composites.
NIST Special Publication 1200-15. Ver 1.0, 16 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-16
15. Scott K, Giannuzzi LA (2015) Strategies for transmission electron microscopy
specimen preparation of polymer composites. NIST Special Publication 1200-16. Ver
1.0, 10 pp. http://dx.doi.org/10.6028/NIST.SP.1200-16
16. Vladár AE (2015) Strategies for scanning electron microscopy sample preparation
and characterization of multiwall carbon nanotube polymer composites. NIST Special
Publication 1200-17. Ver 1.0, 16 pp. http://dx.doi.org/10.6028/NIST.SP.1200-17
17. Nelson BC, Petersen EJ, Jaruga P, Dizdaroglu M (2015) GC/MS measurement of
nanomaterial-induced DNA modifications in isolated DNA. NIST Special Publication
1200-18. Ver 1.0, 13 pp. http://dx.doi.org/10.6028/NIST.SP.1200-18
18. Nelson BC, Petersen EJ, Jaruga P, Dizdaroglu M (2015) GC-MS/MS measurement of
nanomaterial-induced DNA modifications in isolated DNA. NIST Special Publication
1200-19. Ver 1.0, 13 pp. http://dx.doi.org/10.6028/NIST.SP.1200-19
19. Nelson BC, Petersen EJ, Jaruga P, Dizdaroglu M (2015) LC-MS/MS measurement of
nanomaterial-induced DNA modifications in isolated DNA. NIST Special Publication
1200-20. Ver 1.0, 11 pp. http://dx.doi.org/10.6028/NIST.SP.1200-20
20. Murphy KE, Liu J-Y, Montoro Bustos AR, Johnson ME, Winchester MR (2015)
Characterization of nanoparticle suspensions using single particle inductively coupled
plasma mass spectrometry. NIST Special Publication 1200-21. Ver 1.0, 29 pp.
http://dx.doi.org/10.6028/NIST.SP.1200-21
21. Underwood SJ, Gorham JM (2017) Challenges and approaches for particle size
analysis on micrographs of nanoparticles loaded onto textile surfaces. NIST Special
Publication 1200-22. Ver 1.0, 13 pp. https://doi.org/10.6028/NIST.SP.1200-22
22. Johnson ME, et al. (2017) Sucrose density gradient centrifugation for efficient
separation of engineered nanoparticles from a model organism, Caenorhabditis
elegans. NIST Special Publication 1200-24. Ver 1.1, 18 pp.
https://doi.org/10.6028/NIST.SP.1200-24
23. Savelas AR, Yu LL, Jacobs DS, Nguyen T, Sung L (2017) Protocol for collecting and
quantifying release from weathered epoxy-nanosilica coatings: Using a simulated rain
method and inductively coupled plasma-optical emission spectrometry. NIST Special
Publication 1200-25. Ver 1.0, 10 pp. https://doi.org/10.6028/NIST.SP.1200-25
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24. Cho TJ, Hackley VA (2018) Assessing the chemical and colloidal stability of
functionalized gold nanoparticles. NIST Special Publication 1200-26. 13 pp.
https://doi.org/10.6028/NIST.SP.1200-26
NIST-NCL Assay Protocols
Nanotechnology Characterization Laboratory (NCL), National Cancer Institute
https://ncl.cancer.gov/resources/assay-cascade-protocols [accessed 2018 August 17].
1. Grobelny J, et al. (2009) Size measurement of nanoparticles using atomic force
microscopy. NIST - NCL Joint Assay Protocol, PCC-6. Ver 1.1, 2009, 20 pp.
[accessed 2018 July 3].
https://ncl.cancer.gov/sites/default/files/protocols/NCL_Method_PCC-2.pdf
2. Hackley VA, Clogston JD (2010) Measuring the size of nanoparticles in aqueous
media using batch-mode dynamic light scattering. NIST - NCL Joint Assay Protocol,
PCC-1. Ver 1.1, 22 pp. [accessed 2018 July 3].
https://ncl.cancer.gov/sites/default/files/protocols/NCL_Method_PCC-1.pdf
3. Bonevich JE, Haller WK (2010) Measuring the size of nanoparticles using
transmission electron microscopy (TEM). NIST - NCL Joint Assay Protocol, PCC-7.
Ver 1.1, 13 pp. [accessed 2018 July 3].
https://ncl.cancer.gov/sites/default/files/protocols/NCL_Method_PCC-7.pdf
4. Yu LL, Wood LJ, Long SE (2010) Determination of gold in rat tissue with inductively
coupled plasma mass spectrometry. NIST - NCL Joint Assay Protocol, PCC-8. Ver 1.1,
21 pp. [accessed 2018 July 3]. http://nanolab.cancer.gov/NCL_Method_PCC-8.pdf
5. Yu LL, Wood LJ, Long SE (2010) Determination of gold in rat blood with inductively
coupled plasma mass spectrometry. NIST - NCL Joint Assay Protocol, PCC-9. Ver 1.1,
20 pp. [accessed 2018 July 3]. http://nanolab.cancer.gov/NCL_Method_PCC-9.pdf
6. Pease III LF, Tsai D-H, Zangmeister RA, Winchester MR, Tarlov MJ (2010) Analysis
of gold nanoparticles by electrospray differential mobility analysis (ES-DMA). NIST -
NCL Joint Assay Protocol, PCC-10. Ver 1.1, 8 pp. [accessed 2018 July 3].
http://nanolab.cancer.gov/NCL_Method_PCC-10.pdf
7. Winchester MR (2010) Method for determination of the mass fraction of particle-
bound gold in suspensions of gold nanoparticles. NIST - NCL Joint Assay Protocol,
PCC-11. Ver 1.1, 16 pp. [accessed 2018 July 3].
http://nanolab.cancer.gov/NCL_Method_PCC-11.pdf
8. Pratt KW (2010) Measuring the electrolytic conductivity of nanoparticle suspensions.
NIST - NCL Joint Assay Protocol, PCC-12. Ver 1.1, 8 pp. [accessed 2018 July 3].
http://nanolab.cancer.gov/NCL_Method_PCC-12.pdf
9. Pratt KW (2010) Measuring the pH of nanoparticle suspensions. NIST - NCL Joint
Assay Protocol, PCC-13. Ver 1.1, 8 pp. [accessed 2018 July 3].
http://nanolab.cancer.gov/NCL_Method_PCC-13.pdf
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10. Cleveland D (2010) Quantification of free and chelated gadolinium species in
nanoemulsion-based magnetic resonance imaging contrast agent formulations using
hyphenated chromatography methods. NIST - NCL Joint Assay Protocol, PCC-14. Ver
1.0, 24 pp. [accessed 2018 July 3]. http://nanolab.cancer.gov/NCL_Method_PCC-
14.pdf
11. Vladár AE, Ming B (2011) Measuring the size of colloidal gold nano-particles using
high-resolution scanning electron microscopy. NIST - NCL Joint Assay Protocol,
PCC-15. Ver 1.0, 20 pp. [accessed 2018 July 3].
http://nanolab.cancer.gov/NCL_Method_PCC-15.pdf
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Appendix E: Nanoscale Reference Materials
RM: Reference Material; SRM: Standard Reference Material; NP: nanoparticle; CNT:
carbon nanotube
Material
Type Identifier(s) Form Reference
Property
Nominal
Value
Release
Date
Total #
Units
Sold*
gold NPs
RM 8011 in aqueous
suspension
mean
diameter
30 nm 12/17/07 555
RM 8012 60 nm 12/17/07 615
RM 8013 100 nm 12/17/07 613
TiO2 NPs SRM 1898 dry powder
specific
surface
area
55 m2/g 6/14/12 118
silver NPs RM 8017 freeze-dried mean
diameter 75 nm 12/6/14 67
silicon NPs RM 8027 in toluene
suspension
mean
diameter 2 nm 2/4/14 9
single-wall
CNTs
SRM 2483 dry soot mass
fraction
impurity
elements 11/14/11 62
RM 8281 in aqueous
suspension length
"long",
"medium",
"short"
7/9/13 15
multiwall
CNTs SRM 2484 dry soot
mass
fraction
impurity
elements 6/1/17 0
*As of July 2018
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